CN100594183C - Method for preparing titanate based on carnallite and Ti-containing minerals - Google Patents
Method for preparing titanate based on carnallite and Ti-containing minerals Download PDFInfo
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- CN100594183C CN100594183C CN200810023311A CN200810023311A CN100594183C CN 100594183 C CN100594183 C CN 100594183C CN 200810023311 A CN200810023311 A CN 200810023311A CN 200810023311 A CN200810023311 A CN 200810023311A CN 100594183 C CN100594183 C CN 100594183C
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- China
- Prior art keywords
- carnallitite
- titanate
- tio
- kmgcl
- titaniferous ore
- Prior art date
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910052500 inorganic mineral Inorganic materials 0.000 title abstract description 8
- 239000011707 mineral Substances 0.000 title abstract description 8
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 title abstract description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 46
- 239000000203 mixture Substances 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 19
- 239000011734 sodium Chemical group 0.000 claims description 13
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 10
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 claims description 8
- 150000001339 alkali metal compounds Chemical class 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- 239000003575 carbonaceous material Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052792 caesium Chemical group 0.000 claims description 5
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical group [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 5
- 239000000571 coke Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052701 rubidium Inorganic materials 0.000 claims description 5
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical group [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 4
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 4
- 229910052728 basic metal Inorganic materials 0.000 claims description 4
- 150000003818 basic metals Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical group [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Chemical group 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052712 strontium Chemical group 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical group [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 2
- 229910001963 alkali metal nitrate Inorganic materials 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- -1 gac Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 229910021025 KMgCl3 Inorganic materials 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 17
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Chemical compound [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 6
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002783 friction material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Images
Abstract
The invention discloses a method for preparing titanate based on carnallite and titanium-containing mineral, which includes using the carnallite and the titanium-containing mineral as the material, mixing evenly, wherein KMgCl3 and TiO2 respectively stands for the carnallite and the titanium-containing mineral with a mole ratio of KMgCl3: TiO2 at 1:(1-10); calcining at 1200 DEG C for 30 min-12hr;and pulverizing, water washing, filtering and drying to obtain the titanate. By using the low-cost material, the method reduces the reaction temperature, further reduces the production cost, saves theenergy consumption and is suitable for industrial production.
Description
Technical field
The invention belongs to inorganic titanate material field, be specifically related to a kind of method that mainly prepares titanate from carnallitite and titaniferous ore.
Background technology
The inorganic titanate material has important use in daily life and industrial production, can be used as friction materials, and structured materials such as plastics, ceramic reinforcing material use; Can be used as ion-exchange material again, heat insulation heat-stable material, catalytic material, functional materialss such as piezoelectric use.In numerous titanate materials, titanate whisker and platelet are paid close attention to by people because of its excellent performance and high added value.
The titanate whisker is an example with the potassium titanate crystal whisker, and layered titanic acid potassium whisker has ion exchangeable, can be used for the processing of trade effluent; Tunnel-like can be used as fortifying fibre, friction materials, heat insulation heat-stable material, alkaline-resisting material, filter membrane, sensor material etc.Titanate lamella is same use wide, as sorbing material, as the carrier of friction materials, anti-uv materials etc.
The preparation method of existing titanate whisker and platelet has multiple, but its main raw material is often selected Chemicals for use, as the derived product and the various basic metal/alkaline earth metal compound of titanium white industry.Price just because of raw material is higher, makes that the price of titanate whisker and platelet is very expensive, has limited its application scale.
Carnallitite and titaniferous ore all are the nature mineral wealth.The carnallitite molecular formula is KMgCl
36H
2O, the CA registration number is 1318-27-0, is potassium-containing compound, magnesium-containing compound raw materials for production.Titaniferous ore is the raw materials for production of titanium white industry.If can prepare titanate whisker or platelet as main raw material with carnallitite and titaniferous ore, not only improved the comprehensive utilization ratio of mineral wealth, reduce raw materials cost, and shortened the explained hereafter flow process of titanate whisker and platelet, reduced the consumption of energy.Therefore exploitation is the novel process that main raw material prepares titanate whisker and platelet based on carnallitite and titaniferous ore, can reduce the production cost of titanate whisker and platelet, break Price Bottleneck, the application that promotes high-performance titanate whisker and platelet is had great importance.
Summary of the invention
The objective of the invention is directly to utilize nature mineral wealth carnallitite and titaniferous ore to prepare titanate, thereby the preparation method of a kind of low cost, less energy-consumption, the simple titanate of technology is provided.
Purpose of the present invention can reach by following measure:
A kind ofly prepare the method for titanate, may further comprise the steps based on carnallitite and titaniferous ore:
(1) is main raw material with carnallitite and titaniferous ore, mixes;
Wherein carnallitite and titaniferous ore are with KMgCl
3, TiO
2Meter, mol ratio is KMgCl
3: TiO
2=1: (1～10);
(2) with said mixture 800～1200 ℃ of following sintering 30 minutes～12 hours, temperature of reaction is preferably 900～1100 ℃;
(3) sintered product is pulverized, washes, filters, dried, obtain titanate.
Wherein raw material also can comprise alkali metal compound, and wherein carnallitite, titaniferous ore, alkali metal compound are with KMgCl
3, TiO
2, M
2The O meter, mol ratio is KMgCl
3: TiO
2: M
2O=1: (1～10): (1～2), wherein M is a basic metal.
Raw material also can comprise alkaline earth metal compound, and wherein carnallitite, titaniferous ore, alkaline earth metal compound are with KMgCl
3, TiO
2, EO meter, mol ratio is KMgCl
3: TiO
2: EO=1: (1～10): (1～4), wherein E is an alkaline-earth metal.
In raw material, increase in alkali metal compound or the alkaline earth metal compound, can also increase the quality percentage composition and be 0.5%～40% contenting carbon material,, improve the quality of products to regulate the content of each element of the finished product.
(preferably add contenting carbon material simultaneously) when comprising basic metal or alkaline earth metal compound in the raw material, finally can obtain general formula is M
0.68-1Mg
0.15-1.5Ti
0.66-5O
2-11(wherein M is preferably lithium, sodium, rubidium or caesium), M "
0.35-2Fe
0-2.5Ti
0.25-6O
2-13(wherein M " be preferably lithium, sodium, potassium, rubidium or caesium) or E
1-2Fe
0-4Ti
0.25-4O
2-12The whisker or the platelet of the titanate of (wherein E is preferably magnesium, calcium, barium or strontium).When only being raw material, with KMgCl with carnallitite and titaniferous ore
3, TiO
2The meter mol ratio is preferably 1: (1～4); Finally can obtain MgFe
1-2Ti
2.5-4O
7.5-10The whisker of titanate or platelet.The length of the whisker that the present invention obtains is 10～100 μ m, and diameter is 0.2～4 μ m; The arithmetical av of the equivalent length of platelet and equivalent width is 0.1～200 μ m, equivalent length and when to measure wide ratio be 1～5, and its mean thickness is 0.05～10 μ m.Certainly can also add other raw materials or auxiliary agent in the raw material to reach some specific effect.
Wherein titaniferous ore is selected from one or more in ilmenite, ilmenite concentrate, pseudobrookite, ulvite, the red arizonite; Alkali metal compound is selected from one or more of alkali-metal carbonate, nitrate or oxyhydroxide, is preferably carbonate, nitrate or the oxyhydroxide of lithium, sodium, potassium, rubidium or caesium; Alkaline earth metal compound is selected from one or more of oxide compound, carbonate, nitrate or oxyhydroxide of alkaline-earth metal, is preferably carbonate, nitrate or the oxyhydroxide of calcium, strontium or barium; Contenting carbon material is selected from one or more of graphite, gac, coke or coal.
Beneficial effect of the present invention:
This law uses nature mineral wealth carnallitite and titaniferous ore to prepare titanate whisker or platelet as main raw material, and its production cost is very cheap, and the crystal good forming effect is fit to industrial production.
Description of drawings
Fig. 1 is: Li of the present invention
0.85Mg
0.15Ti
2O
4Scanning electronic microscope (SEM) figure.
Fig. 2 is: Na of the present invention
0.35Fe
0.69Ti
3.34O
8Scanning electronic microscope (SEM) figure.
Fig. 3 is: BaFe of the present invention
2Ti
4O
12Scanning electronic microscope (SEM) figure.
Embodiment
Embodiment 1
With carnallitite, ulvite, CsOH, with KMgCl
3, TiO
2, Cs
2The O meter, mol ratio is KMgCl
3: TiO
2: Cs
2O=1: 10: 1 mixed, other adds graphite 40wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain CsMg at 1200 ℃ of following sintering 30min
0.5Ti
5O
11Whisker, its length are 20～40m, and diameter is 0.6～1.5 μ m.
With carnallitite, red arizonite, Na
2CO
3And NaNO
3, with KMgCl
3, TiO
2, Na
2The O meter, mol ratio is KMgCl
3: TiO
2: Na
2O=1: 5: 2 mixed, other adds gac 30wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain Na at 800 ℃ of following sintering 12h
0.68Mg
0.34Ti
0.66O
2Platelet, its equivalent mean value are 1～5 μ m, equivalent length and when to measure wide ratio be 1.5, and thickness is 0.5～2 μ m (equivalent mean value=(equivalent length+equivalent width)/2).
Embodiment 3
With carnallitite, red arizonite, Li
2CO
3, with KMgCl
3, TiO
2, Li
2The O meter, mol ratio is KMgCl
3: TiO
2: Li
2O=1: 1: 2 mixed, other adds gac, coke 35wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain Li at 900 ℃ of following sintering 7h
0.85Mg
0.15Ti
2O
4Whisker, its length are 20～60 μ m, and diameter is 1.5～2.5 μ m.
Embodiment 4
With carnallitite, ilmenite concentrate, CsOH, with KMgCl
3, TiO
2, Cs
2The O meter, mol ratio is KMgCl
3: TiO
2: Cs
2O=1: 2: 2 mixed, other adds coke 3wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain Cs at 900 ℃ of following sintering 5h
0.75Fe
0.75Ti
0.25O
2Whisker, its length are 10～40 μ m, and diameter is 0.5～2 μ m.
Embodiment 5
With carnallitite, ilmenite, Li
2CO
3, with KMgCl
3, TiO
2, Li
2The O meter, mol ratio is KMgCl
3: TiO
2: Li
2O=1: 3: 2 mixed, other adds graphite 0.5wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain LiFe at 1100 ℃ of following sintering 6h
2.5Ti
3O
9Platelet, its equivalent mean value are 0.5～10 μ m, equivalent length and when to measure wide ratio be 2, and thickness is 0.1～2 μ m.
Embodiment 6
With carnallitite, red arizonite, NaOH, with KMgCl
3, TiO
2, Na
2The O meter, mol ratio is KMgCl
3: TiO
2: Na
2O=1: 10: 1 mixed.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain Na at 800 ℃ of following sintering 12h
0.35Fe
0.69Ti
3.34O
8Platelet, its equivalent mean value are 100～200 μ m, equivalent length and when to measure wide ratio be 2.5, and thickness is 5～10 μ m.
Embodiment 7
With carnallitite, red arizonite, BaCO
3, with KMgCl
3, TiO
2, BaO meter, mol ratio is KMgCl
3: TiO
2: BaO=1: 10: 2.5 mixed.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain BaFe at 1000 ℃ of following sintering 4h
2Ti
4O
12Platelet, its equivalent mean value are 0.1～10 μ m, equivalent length and when to measure wide ratio be 1.5, and thickness is 0.05～0.5 μ m.
Embodiment 8
With carnallitite, pseudobrookite, CaCO
3, with KMgCl
3, TiO
2, CaO meter, mol ratio is KMgCl
3: TiO
2: BaO=1: 4: 1 mixed, other adds graphite 5wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain CaFe at 950 ℃ of following sintering 9h
0.66Ti
0.33O
2.66Whisker, its length are 50～100 μ m, and diameter is 2.5～4 μ m.
Embodiment 9
With carnallitite, pseudobrookite, Sr (OH)
2And Sr (NO
3)
2, with KMgCl
3, TiO
2, SrO meter, mol ratio is KMgCl
3: TiO
2: SrO=1: 2: 4 mixed, other adds graphite 5wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain SrFe at 900 ℃ of following sintering 10h
0.5Ti
0.5O
2.775Platelet, its equivalent mean value are 80～200 μ m, equivalent length and when to measure wide ratio be 3, and thickness is 6～10 μ m.
Embodiment 10
With carnallitite, ilmenite concentrate, ilmenite, with KMgCl
3, TiO
2Meter, mol ratio is KMgCl
3: TiO
2=1: 8 mixed.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain MgFeTi at 1200 ℃ of following sintering 3h
4O
10Platelet, its equivalent mean value are 60～100 μ m, equivalent length and when to measure wide ratio be 5, and thickness is 3～5 μ m.
Embodiment 11
With carnallitite, ulvite, with KMgCl
3, TiO
2Meter, mol ratio is KMgCl
3: TiO
2=1: 1 mixed.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain MgFeTi at 1100 ℃ of following sintering 4h
2.5O
7.5Whisker, its length are 20～40 μ m, and diameter is 0.6～1.2 μ m.
Embodiment 12
With carnallitite, pseudobrookite and red arizonite, with KMgCl
3, TiO
2Meter, mol ratio is KMgCl
3: TiO
2=1: 3 mixed.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain MgFe at 900 ℃ of following sintering 5h
2Ti
3O
10Platelet, its equivalent mean value are 30～50 μ m, equivalent length and when to measure wide ratio be 3, and thickness is 1.5～2.5 μ m.
Embodiment 13
With carnallitite, ilmenite, KNO
3, with KMgCl
3, TiO
2, K
2The O meter, mol ratio is KMgCl
3: TiO
2: K
2O=1: 6: 1 mixed, other adds graphite 30wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried 4 hours down at 180 ℃, obtain K at 1000 ℃ of following sintering 4h
2Ti
6O
13Whisker, its length are 10～20 μ m, and diameter is 0.2～0.5 μ m.
Embodiment 14
The just brilliant ore deposit of carnallitite, titanium, BaO are with KMgCl
3, TiO
2, BaO meter, mol ratio is KMgCl
3: TiO
2: BaO=1: 1: 1 mixed, other adds graphite 40wt%.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain BaTiO at 1200 ℃ of following sintering 4h
3Platelet, its equivalent mean value are 0.1～5 μ m, equivalent length and when to measure wide ratio be 1.5, and thickness is 0.05～0.5 μ m.
Comparative example 1
With ilmenite concentrate, CsOH, with TiO
2, Cs
2The O meter, mol ratio is TiO
2: Cs
2O=1: 1 mixed, other adds coke 20wt% and CsCl 5wt% as fused salt, and mixture is placed High Temperature Furnaces Heating Apparatus, at 900 ℃ of following sintering 5h, sintered product is pulverized, washes, filters, is dried, and obtains Cs
0.75Fe
0.75Ti
0.25O
2Particle.
The CsCl that compares employing with embodiment 4 is as fused salt, but effect is nothing like carnallitite, and its production cost exceeds about 5 times than embodiment 4.
Comparative example 2
With BaCO
3, Fe
2O
3, TiO
2With mol ratio is 1: 1: 4 mixed, and mixture is placed High Temperature Furnaces Heating Apparatus, at 1250 ℃ of following sintering 25h, sintered product is pulverized, washes, filters, is dried, and obtains BaFe
2Ti
4O
12Platelet.Its equivalent mean value 0.1～10 μ m, equivalent length and when to measure wide ratio be 1.5, thickness 0.05～0.5 μ m.
Compare with embodiment 7, owing to do not add carnallitite, the sintering temperature of product has improved 250 ℃, Fe
2O
3And TiO
2Use, make production cost about 2 times than exceeding of embodiment 7.
Comparative example 3
With MgO, Fe
2O
3, TiO
2, be 2: 1: 2 mixed with mol ratio.Mixture is placed High Temperature Furnaces Heating Apparatus,, sintered product is pulverized, washes, filters, dried, obtain MgFeTi at 1100 ℃ of following sintering 4h
2.5O
7.5Particle.
Owing to do not add carnallitite, lacked corresponding flux with embodiment 11, product is a particle.
Reference:
[1] Lu Xiaohua, He Ming, Yang Zhuhong etc., a kind of high-specific surface area titanium oxide synthetic method, ZL03158274.5
[2] Feng Xin, Lv Jiazhen, Lu Xiaohua etc. the application [J] of potassium titanate crystal whisker in matrix material. matrix material journal, 1999,16 (4): 1-7.
[3]J.T.Zeng，K.W.Kwok，w?W.K.Tam，et?al.Plate?like?Na
0.5Bi
0.5TiO
3?template?synthesizedby?a?topochemical?method[J].Journal?of?the?American?Ceramic?Society，2006，89(12)：3850-3853.
[4] Lu Xiaohua, Liu Chang, Qin Xifeng etc., the preparation method of a kind of basic metal base whisker and platelet, CN200610039687.5
[5] coulee is rich, and bridge is grown the man, and well is stretched tree, Lepidocrosite type potassium magnesium titanate and preparation method thereof, ZL01813460.2
[6]A.M.El-Toni，Y.S，T.S.Particle?size?control?of?plate-like?lepidocrocite-related?potassiumlithium?titanate?through?optimization?of?synthesis?parameters[J].Materials?Letters，2006，60：185-189
[7] Feng Xin, Yang Zhuhong, Lu Xiaohua etc., the manufacture method of crystal whisker of hexa potassium titanate, ZL00112275.4
[8] Huai gift, Zhao Kuanfang, the preparation method of crystal whisker of hexa potassium titanate, ZL93111038.6
[9] Lu Xiaohua, sudden and violent peaceful clock, Feng Xin, the manufacture method of crystal whisker of hexa potassium titanate and fiber, ZL99114005.2
[10] Huai gift, Zhao Kuanfang, a kind of preparation method of titanate lamella, CN200510047963.
Claims (7)
1, a kind ofly prepare the method for titanate, it is characterized in that may further comprise the steps based on carnallitite and titaniferous ore:
(1) is main raw material with carnallitite and titaniferous ore, mixes;
Wherein carnallitite and titaniferous ore are with KMgCl
3, TiO
2Meter, mol ratio is KMgCl
3: TiO
2=1: 1～10;
Comprise alkali metal compound or alkaline earth metal compound in the raw material, wherein carnallitite, titaniferous ore, alkali metal compound are with KMgCl
3, TiO
2, M
2O meter mol ratio is KMgCl
3: TiO
2: M
2O=1: 1～10: 1～2, carnallitite, titaniferous ore, alkaline earth metal compound are with KMgCl
3, TiO
2, EO meter mol ratio is KMgCl
3: TiO
2: EO=1: 1～10: 1～4, wherein M is a basic metal, E is an alkaline-earth metal;
(2) with said mixture 800～1200 ℃ of following sintering 30 minutes～12 hours;
(3) sintered product is pulverized, washes, filters, dried, obtain titanate.
2, according to claim 1ly prepare the method for titanate based on carnallitite and titaniferous ore, it is characterized in that described raw material also comprises contenting carbon material, wherein the quality percentage composition of contenting carbon material is 0.5%～40%.
3, according to claim 1ly prepare the method for titanate, it is characterized in that described titaniferous ore is selected from one or more in ilmenite, ilmenite concentrate, pseudobrookite, ulvite, the red arizonite based on carnallitite and titaniferous ore.
4, according to claim 1ly prepare the method for titanate, it is characterized in that described alkali metal compound is selected from one or more of alkali-metal carbonate, nitrate or oxyhydroxide based on carnallitite and titaniferous ore.
5, according to claim 1ly prepare the method for titanate, it is characterized in that described alkaline earth metal compound is selected from one or more of the oxide compound of alkaline-earth metal, carbonate, nitrate or oxyhydroxide based on carnallitite and titaniferous ore.
6, according to claim 2ly prepare the method for titanate, it is characterized in that described contenting carbon material is selected from one or more of graphite, gac, coke or coal based on carnallitite and titaniferous ore.
7, according to claim 1ly prepare the method for titanate, it is characterized in that described titanate is M based on carnallitite and titaniferous ore
0.68-1Mg
0.15-1.5Ti
0.66-5O
2-11, M "
0.35-2Fe
0-2.5Ti
0.25-6O
2-13Or E
1-2Fe
0-4Ti
0.25-4O
2-12Whisker or platelet, wherein M is lithium, sodium, rubidium or caesium, M, and " be lithium, sodium, potassium, rubidium or caesium, E is magnesium, calcium, barium or strontium.
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| 六钛酸钾晶须制备新工艺. 胡恒瑶等.中国有色金属学报，第14卷第专辑1期. 2004 |
| 六钛酸钾晶须制备新工艺. 胡恒瑶等.中国有色金属学报，第14卷第专辑1期. 2004 * |
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